Professional Documents
Culture Documents
Keywords: Sewage sludge ash (SSA) is obtained from wastewater sludge incineration, and it can be recycled
Sewage sludge ash in cement-based materials. The environmental conditions show significant influence on the vol-
Volume deformation ume deformation of cement-based materials with SSA. So in this study, the effect of environmen-
Environmental condition tal conditions on the volume deformation of mortars with SSA was investigated, and the underly-
Microstructure
ing mechanism was preliminarily studied with isothermal calorimetry, X-ray diffraction (XRD)
and thermogravimetry (TG). The results indicated that, under seal condition, SSA caused obvious
expansion after the rapid shrinkage at very early age, and reduced the 28d autogenous shrinkage
of mortars. Under drying condition, the addition of SSA enlarged the drying shrinkage of mortars.
Under water immersed condition, the mortars expanded before the age of 7d, and more SSA led
to more obvious expansion. The addition of SSA resulted in more ettringite formed in mortars un-
der sealed and water immersed conditions, leading to the expansion of mortars. The findings of
this study could help to control the volume deformation of mortars with SSA.
1. Introduction
The sewage sludge ash (SSA) is the residue of wastewater sludge after incineration treatment. SSA can be recycled in building ma-
terials, e.g. cement, bricks, ceramic and glass, mortars and concretes [1–3]. In cement-based materials (e.g. mortars and concretes),
SSA can be used to replace partial cement. Previous studies showed that SSA also exhibited pozzolanic reactivity as fly ash did [4]. So
SSA could be used in cement-based materials as supplementary cementitious materials. Replacing partial cement with SSA is also
helpful to reduce the cement usage, lower the carbon emission and avoid the unfavorable effect of SSA on the environments.
Some studies have worked on the influence of SSA on the basic properties of mortars or concretes [3]. The addition of SSA would
reduce the fluidity and mechanical properties of cement-based materials [5–7]. The porosity of cement-based materials was increased
if SSA was added [8–10]. So the addition of SSA also influences the durability of mortars and concretes, such as carbonation, chloride
resistance and freeze-thaw performance [8]. The negative influence of SSA on the properties of mortars or concretes could be reme-
died by several methodologies, such as using nano-materials, improving cement content, refining the SSA particles, etc. [4,11]. The
addition of SSA also influences the volume deformation of mortars and concretes. Tay found that the drying shrinkage of concrete was
* Corresponding author. College of Civil Engineering, Zhejiang University of Technology, Hangzhou, 310023, China.
E-mail address: yangyang@zjut.edu.cn (Y. Yang).
https://doi.org/10.1016/j.jobe.2022.105720
Received 17 June 2022; Received in revised form 16 November 2022; Accepted 7 December 2022
Available online 10 December 2022
2352-7102/© 2022 Elsevier Ltd. All rights reserved.
C. Gu et al. Journal of Building Engineering 65 (2023) 105720
slightly reduced with the increase of SSA content [12]. The drying shrinkage decreased from 855 με to 765 με when 20% cement was
replaced by SSA. But Sasaoka et al. found that the drying shrinkage of concrete with 10% SSA was about 1.5 times to that of control
concrete [13]. Chen et al. also found that the replacement of 20% cement with SSA enlarged the drying shrinkage of mortars by about
25%, and SSA with smaller size resulted in higher drying shrinkage [4,14]. Li et al. tried to recycle SSA in cement mortars. They also
found that the drying shrinkage of mortars was increased due to the presence of SSA [15].
Because of the different composition of wastewater sludge and the different treatment methods, some SSA may contain high con-
tent of sulfates [5,7]. The sulfates in cement-based system may cause the problem of volume instability to cement-based materials,
and would make the volume deformation of cement-based materials more sensitive to the environmental conditions. Garcés et al. in-
vestigated the effect of SSA with high sulfate content on the volume deformation of mortars under different humidities [5]. The SO3
content in SSA was 11.1%. The shrinkage of mortars with 10% SSA and without SSA under 65% RH showed very little difference, and
under 100% RH, mortars with 10% SSA did not show evident expansion. But the study of Gu et al. showed the presence of sulfate-rich
SSA, whose SO3 content was higher than 20.0%, caused obvious expansion of cement paste under water-immersed conditions [7].
Generally, the studies on the volume deformation of cement mortars and concretes with SSA mainly focused on drying shrinkage,
and very few studies were concerned about the autogenous shrinkage and volume deformation under other environments. The envi-
ronmental conditions would show significant influence on the volume deformation of cement mortars and concretes with SSA, espe-
cially for SSA with high sulfate contents. In order to control the volume deformation and reduce the cracking risk of cement-based
materials with SSA, this study aimed to reveal the influence of environmental conditions on the volume deformation of cement mor-
tars with SSA, and tried to uncover the micro-mechanism of volume deformation of mortars with SSA. In this study, mortars with dif-
ferent SSA contents (0%, 5%, 10% and15%) were prepared, and the effect of SSA contents on fluidity and compressive strength of
mortars were studied. Moreover, the length changes of mortar specimens with SSA under different environmental conditions (drying
condition, sealed condition and immersion in water) were measured, and the micro-mechanism on the volume deformation of mor-
tars with SSA was also studied with isothermal calorimetry, X-ray diffraction (XRD) and thermogravimetry (TG).
Table 1
The chemical compositions of cement and SSA (%).
2
C. Gu et al. Journal of Building Engineering 65 (2023) 105720
Table 2
Mix proportions of mortars.
25 mm × 25 mm × 285 mm, and the comparator was used to measure the length change of the specimens from 1d to 28d. The de-
tailed test methods were the same as that used in Ref. [9].
Isothermal calorimetry was applied to study the early age hydration process of mortars. The paste without sand was used as sam-
ples, and the tests were performed at 20 °C under sealed condition, with a TAM air isothermal calorimeter. XRD and TG analysis were
applied to detect the formation of ettringite in mortars. The generation of ettringite significantly influences the volume deformation
of the mortars. The paste powders were used as samples for XRD and TG analysis. The pastes were demolded at 1d, and then were
cured in water at 20 ± 2 °C for the designated ages. Then the paste specimens were crushed into pieces and immersed in acetone to
terminate the cement hydration. After that, they were ground into powders and dried in a vacuum oven with a temperature at 50 °C
for 3 days before the XRD and TG/DSC analysis. XRD analysis was conducted on paste powders with a PANalytical X'Pert PRO powder
diffractometer and a Cu Kα radiation source. The scan range was 5°–80°, the scan rate was 5°/min, the working voltage was 40 kV and
working current was 30 mA. TG analysis was performed with Mettler-Toledo TGA 2. The temperature range was from 40 °C to 300 °C,
and the heating rate was 10 °C/min.
3
C. Gu et al. Journal of Building Engineering 65 (2023) 105720
4
C. Gu et al. Journal of Building Engineering 65 (2023) 105720
tios were 0.5 and 0.6, the effect of SSA content on the compressive strength of mortars were similar to that when water to binder ratio
was 0.4. The low reactivity of SSA was the reason for the compressive strength reduction of mortars [4]. Besides, the presence of SSA
normally enlarges the porosity of cement-based materials, so the strength decreased [10].
5
C. Gu et al. Journal of Building Engineering 65 (2023) 105720
The influence of water to binder ratio on the autogenous shrinkage of mortars with different SSA contents is shown in Fig. 5. The
control mortar with lower water to binder ratio showed higher autogenous shrinkage, which was consistent with the results in most
literatures [26,27]. But for mortars with SSA, the autogenous shrinkage of mortars with SSA was enlarged at higher water to binder
ratio. When SSA content was 15%, the 28d strain of mortar with water to binder ratio at 0.4 was 19 με and it was −70 με for mortar
with water to binder ratio at 0.6. It indicated that the expansion caused by ettringite generation was more pronounced in mortars
with low water to binder ratio. The mortar with water to ratio at 0.6 has a higher porosity, and thus some of the generated ettringite
filled in the pores first and resulted in lower expansion [28]. While, the mortar with water to binder ratio at 0.4 has a denser mi-
crostructure, so the formation of ettringite will cause higher expansion stress in the mortar, and resulted in more pronounced expan-
sion [29].
6
C. Gu et al. Journal of Building Engineering 65 (2023) 105720
sion, the water supply in mortar was sufficient, so more ettringite could be generated when more SSA was added in mortars. When the
water to binder ratio was 0.4, at 7d, the expansive strains of mortars with 0%, 5%, 10% and 15% SSA were 60 με, 77 με, 104 με and
128 με respectively. After 7d, the expansive strains of mortars became almost constant.
The influence of water to binder ratio on the volume deformation of mortars in water is shown in Fig. 9. Generally, the raise of wa-
ter to binder ratio reduced the expansion of mortars in water, and the influence was more significant when the SSA content was
higher. More SSA in mortar caused higher expansion at a lower water to binder ratio. The mortar with a water to binder ratio at 0.4
has denser microstructure, so the formed ettringite would cause more significant expansion [29].
7
C. Gu et al. Journal of Building Engineering 65 (2023) 105720
Fig. 9. Influence of water to binder ratio on the deformation of mortars in water at 28d
8
C. Gu et al. Journal of Building Engineering 65 (2023) 105720
Fig. 10. Hydration heat release of pastes with and without SSA.
from 22 h to 96 h and became much less evident. For mortar with 15% SSA, the second peak was not observed before 168h, which im-
plied excess sulfate was existed. The delayed “sulfate depletion peak” indicated that more ettringite was formed, and thus the expan-
sion of mortars with higher SSA contents was more pronounced during the autogenous shrinkage tests.
Fig. 11. XRD patterns of pastes with 0% and 15% SSA at 7d and 28d (water to binder ratio at 0.5).
9
C. Gu et al. Journal of Building Engineering 65 (2023) 105720
Fig. 12. TG curves of pastes with 15% SSA at 28d under different environments.
TG curves of 15%SSA pastes with water to binder ratios at 0.4 and 0.5 at 28d are show in Fig. 14. TG analysis was not performed
on pastes with water to binder ratio at 0.6 due to the serious bleeding when preparing the samples. Fig. 14 showed that the more et-
tringite was formed in 15%SSA paste with water to binder ratio at 0.5. More water and more pore space are benefit for the formation
of ettringite [37]. Due to the dense microstructure of mortars with water to binder ratio at 0.4, the less ettringite caused more signifi-
cant expansion [29].
Fig. 14. TG curves of 15%SSA mortars with different water to binder ratios at 28d
10
C. Gu et al. Journal of Building Engineering 65 (2023) 105720
4. Conclusions
In this paper, the fluidity and compressive strength of mortars with SSA were studied, the effect of environmental conditions on
the volume deformation of mortars with SSA was investigated, and the micro-mechanism was preliminarily studied. The main conclu-
sions are as follows:
(1) The addition of up to 15% SSA reduced the fluidity of mortars. The reduction was more pronounced when the water to binder
ratio was higher. The addition of up to 15% SSA also slightly reduced the compressive strength of mortars. The compressive
strength reduction was less than 15.0% at 3d and less than 10.0% at 90d.
(2) Under sealed condition, the autogenous shrinkage of mortars developed very fast during 5 h–10 h after the final setting.
Then, the mortars started to expand for about 1.5d–4.5d. The addition of SSA prolonged the expansion duration and enlarged
the expansion strain, and the expansion was more pronounced when the water to binder ratio was lower. After expansion, the
mortars continued to shrink. The 28d autogenous shrinkage of mortars with SSA was reduced when SSA content was higher
and the water to binder ratio was lowered.
(3) Under drying condition, the drying shrinkage of mortars was enlarged when SSA was added, and the enlargement of drying
shrinkage was more pronounced when the water to binder ratio was higher. The decline of water to binder ratio reduced the
drying shrinkage of mortars, and the reduction was more obvious when SSA contents was higher.
(4) Under water immersed condition, the mortars expanded before 7d. The expansion was more remarkable when the water to
binder ratio was lower and SSA content was higher. After 7d, the expansive strains of mortars were almost constant.
(5) The addition of SSA reduced the early age hydration heat release, and postponed the “sulfate depletion peak”. When SSA
content was 15%, the “sulfate depletion peak” was not noticeable before 168h. More ettringite was formed in mortars with
SSA, compared with the control mortar. The ettringite in mortars under drying condition was much less than those under
sealed and water immersed conditions, and ettringite in mortar under water immersed condition was a little more than that
under sealed condition.
The findings of this study could guide the recycle use of SSA in cement mortars, and could help to design the curing regime for
mortars with SSA. Further studies are still needed to reveal the ettringite formation process and the in-depth expansion mechanism of
cement-based materials with SSA.
Data availability
Data will be made available on request.
Acknowledgement
This work was supported by Zhejiang Provincial Natural Science Foundation of China [grant number LY22E080014], China Post-
doctoral Science Foundation [Grant number 2021M692869], the Key Research and Development Program of Zhejiang Province
[grant number 2021C01060], the National Natural Science Foundation of China [grant number 51708502, 52008210], and Innova-
tion and Entrepreneurship Training Program for University Students of Zhejiang University of Technology.
References
[1] C.J. Lynn, R.K. Dhir, G.S. Ghataora, R.P. West, Sewage sludge ash characteristics and potential for use in concrete, Construct. Build. Mater. 98 (2015) 767–779,
https://doi.org/10.1016/j.conbuildmat.2015.08.122.
[2] L. Świerczek, B.M. Cieślik, P. Konieczka, Challenges and opportunities related to the use of sewage sludge ash in cement-based building materials – a review, J.
Clean. Prod. 287 (2021) 125054–125065, https://doi.org/10.1016/j.jclepro.2020.125054.
[3] M. Smol, J. Kulczycka, A. Henclik, K. Gorazda, Z. Wzorek, The possible use of sewage sludge ash (SSA) in the construction industry as a way towards a circular
economy, J. Clean. Prod. 95 (2015) 45–54, https://doi.org/10.1016/j.jclepro.2015.02.051.
[4] Z. Chen, C.S. Poon, Comparative studies on the effects of sewage sludge ash and fly ash on cement hydration and properties of cement mortars, Construct.
Build. Mater. 154 (2017) 791–803, https://doi.org/10.1016/j.conbuildmat.2017.08.003.
[5] P. Garcés, M. Pérez Carrión, E. García-Alcocel, J. Payá, J. Monzó, M.V. Borrachero, Mechanical and physical properties of cement blended with sewage sludge
ash, Waste Manage. (Tucson, Ariz.) 28 (12) (2008) 2495–2502, https://doi.org/10.1016/j.wasman.2008.02.019.
[6] C. Fu, S. Li, R. He, K. Zhou, Y. Zhang, Chloride profile characterization by electron probe microanalysis, powder extraction and AgNO3 colorimetric: a
comparative study, Construct. Build. Mater. 341 (2022) 127892, https://doi.org/10.1016/j.conbuildmat.2022.127892.
[7] C. Gu, Y. Ji, Y. Zhang, Y. Yang, J. Liu, T. Ni, Recycling use of sulfate-rich sewage sludge ash (SR-SSA) in cement-based materials: assessment on the basic
properties, volume deformation and microstructure of SR-SSA blended cement pastes, J. Clean. Prod. 282 (2021) 124511–124523, https://doi.org/10.1016/
11
C. Gu et al. Journal of Building Engineering 65 (2023) 105720
j.jclepro.2020.124511.
[8] B. Krejcirikova, C. Rode, R. Peuhkuri, Determination of hygrothermal properties of cementitious mortar: the effect of partial replacement of cement by
incinerated sewage sludge ash, J. Build. Phys. 42 (2) (2018) 771–787, https://doi.org/10.1177/1744259118791202.
[9] C. Gu, Y. Ji, J. Yao, Y. Yang, J. Liu, T. Ni, H. Zhou, Y. Tong, X. Zhang, Feasibili-ty of recycling sewage sludge ash in ultra-high performance concrete: volume
deformation, microstructure and ecological evaluation, Construct. Build. Mater. 318 (2022) 125823–125834, https://doi.org/10.1016/
j.conbuildmat.2021.125823.
[10] B. Krejcirikova, L.M. Ottosen, G.M. Kirkelund, C. Rode, R. Peuhkuri, Characterization of sewage sludge ash and its effect on moisture physics of mortar, J.
Build. Eng. 21 (2019) 396–403, https://doi.org/10.1016/j.jobe.2018.10.021.
[11] D.F. Lin, K.L. Lin, W.C. Chang, H.L. Luo, M.Q. Cai, Improvements of nano-SiO2 on sludge/fly ash mortar, Waste Manage. (Tucson, Ariz.) 28 (6) (2008)
1081–1087, https://doi.org/10.1016/j.wasman.2007.03.023.
[12] J.H. Tay, Sludge ash as filler for portland cement concrete, J. Environ. Eng. 113 (2) (1987) 345–351, https://doi.org/10.1061/(ASCE)0733-9372(1987)113:2
(345).
[13] N. Sasaoka, K. Yokoi, T. Yamanaka, Basic study of concrete made using ash derived from the incinerating sewage sludge, Int. J. Mod. Phys. B 20 (25n27) (2008)
3716–3721, https://doi.org/10.1142/S0217979206040258.
[14] Z. Chen, C.S. Poon, Comparing the use of sewage sludge ash and glass powder in cement mortars, Environ. Technol. 38 (11) (2017) 1390–1398, https://
doi.org/10.1080/09593330.2016.1230652.
[15] J.S. Li, M.Z. Guo, Q. Xue, C.S. Poon, Recycling of incinerated sewage sludge ash and cathode ray tube funnel glass in cement mortars, J. Clean. Prod. 152
(2017) 142–149, https://doi.org/10.1016/j.jclepro.2017.03.116.
[16] GB 175-2007, Common Portland Cement, Standardization Administration of the People’s Republic of China, Beijing, China, 2007.
[17] ISO 679:2009, Methods of Testing Cements-Determination of Strength, International Organization for Standardization, Switzerland, 2009.
[18] GB/T 2419-2005, Test Method for Fluidity of Cement Mortar, Standardization Administration of the People’s Republic of China, Beijing, China, 2005.
[19] GB/T 17671-1999, Method of Testing Cement-Determination of Strength, Standardization Administration of the People’s Republic of China, Beijing, China,
1999.
[20] ASTM Standard C1698-14, Standard Test Method for Autogenous Strain of Cement Paste and Mortar, ASTM International, West Conshohocken, USA, 2014.
[21] ASTM Standard C596-17, Standard Test Method for Drying Shrinkage of Mortar Containing Hydraulic Cement, ASTM International, West Conshohocken, USA,
2017.
[22] ASTM Standard C1698-17, Standard Test Method for Potential Expansion of Portland- Cement Mortars Exposed to Sulfate, ASTM International, West
Conshohocken, USA, 2015.
[23] Y. Yang, L. Ma, J. Huang, C. Gu, Z. Xu, J. Liu, T. Ni, Evaluation of the thermal and shrinkage stresses in restrained high-performance concrete, Materials 12 (22)
(2019) 3680–3694, https://doi.org/10.3390/ma12223680.
[24] C. Gu, W. Sun, L. Guo, Q. Wang, J. Liu, Y. Yang, Investigation of microstructural damage in ultrahigh-performance concrete under freezing-thawing action,
Adv. Mater. Sci. and Eng. 2018 (2018) 3701682, https://doi.org/10.1155/2018/3701682.
[25] L. Wu, N. Farzadnia, C. Shi, Z. Zhang, H. Wang, Autogenous shrinkage of high performance concrete: a review, Construct. Build. Mater. 149 (2017) 62–75,
https://doi.org/10.1016/j.conbuildmat.2017.05.064.
[26] S. Tang, D. Huang, Z. He, A review of autogenous shrinkage models of concrete, J. Build. Eng. 44 (2021) 103412, https://doi.org/10.1016/
j.jobe.2021.103412.
[27] R. He, S. Li, C. Fu, K. Zhou, Z. Dong, Influence of cyclic drying–wetting and carbonation on oxygen diffusivity of cementitious materials: interpretation from the
perspective of microstructure, J. Mater. Civ. Eng. 34 (2022) 04022256, https://doi.org/10.1061/(ASCE)MT.1943-5533.0004414.
[28] G.J. Yin, Z.Q. Shan, L. Miao, Y.J. Tang, X.B. Zuo, X.D. Wen, Finite element analysis on the diffusion-reaction-damage behavior in concrete subjected to sodium
sulfate attack, Eng. Fail. Anal. 137 (2022) 106278, https://doi.org/10.1016/j.engfailanal.2022.106278.
[29] P. Carballosa, J.L.G. Calvo, D. Revuelta, Influence of expansive calcium sulfoaluminate agent dosage on properties and microstructure of expansive self-
compacting concretes, Cement Concr. Compos. 107 (2020) 103464, https://doi.org/10.1016/j.cemconcomp.2019.103464.
[30] H. Prayuda, R. Dumaru, G. Tanapornraweekit, S. Tangtermsirikul, W. Saengsoy, K. Matsumoto, Estimation of restrained expansion strain of reinforced
expansive concrete considering mixture and curing conditions, Construct. Build. Mater. 322 (2022) 126386, https://doi.org/10.1016/
j.conbuildmat.2022.126386.
[31] N.P. Tran, C. Gunasekara, D.W. Law, S. Houshyar, S. Setunge, A. Cwirzen, A critical review on drying shrinkage mitigation strategies in cement-based
materials, J. Build. Eng. 38 (2021) 102210–102226, https://doi.org/10.1016/j.jobe.2021.102210.
[32] P.K. Mehta, P.J.M. Monteiro, Concrete: Microstructure, Properties, and Materials, fourth ed., McGraw-Hill, 2013.
[33] C. Hesse, F. Goetz-Neunhoeffer, J. Neubauer, A new approach in quantitative in-situ XRD of cement pastes: correlation of heat flow curves with early hydration
reactions, Cement Concr. Res. 41 (1) (2011) 123–128, https://doi.org/10.1016/j.cemconres.2010.09.014.
[34] D. Jansen, F. Goetz-Neunhoeffer, B. Lothenbach, J. Neubauer, The early hydration of Ordinary Portland Cement (OPC): an approach comparing measured heat
flow with calculated heat flow from QXRD, Cement Concr. Res. 42 (1) (2012) 134–138, https://doi.org/10.1016/j.cemconres.2011.09.001.
[35] ASTM-C1679, Standard Practice for Measuring Hydration Kinetics of Hydraulic Cementitious Mixtures Using Isothermal Calorimetry, West Conshohocken,
USA, 2017.
[36] H. Li, Y. Liu, C. Xu, X. Guan, D. Zou, G. Jing, Synergy effect of synthetic ettringite modified by citric acid on the properties of ultrafine sulfoaluminat cement-
based materials, Cement Concr. Compos. 125 (2022) 104312–104318, https://doi.org/10.1016/j.cemconcomp.2021.104312.
[37] I. Odler, J. Colánsubauste, Investigations on cement expansion associated with ettringite formation, Cement Concr. Res. 29 (5) (1999) 731–735, https://
doi.org/10.1016/S0008-8846(99)00048-4.
12